Determination of kava lactones in food supplements by liquid chromatography-atmospheric pressure chemical ionisation tandem mass spectrometry

Reversed-phase liquid chromatography and detection with atmospheric pressure chemical ionisation tandem mass spectrometry was used for the determination of kava extracts in herbal mixtures. One percent of kava extract can be detected, corresponding to approximately 0.05-0.2 mg/g of the individual kava lactones kavain, dihydrokavain, yangonin, desmethoxyyangonin, methysticin and dihydromethysticin. Reliable quantification is obtained from concentrations of 0.25-1 mg/g, depending on the compound. At these concentration levels, the relative standard deviations were 10-14%. Validation showed good linearity and recoveries for all the kava lactones with the exception of yangonin. During method development, degradation of yangonin was observed. The degradation product was identified by nuclear magnetic resonance (NMR) as cis-yangonin. The method was applied to the analysis of commercial herbal products available in the Dutch market before and after market restrictions of kava-containing preparations. The results showed that even though 'old' products contained kava extract, the new formulations were negative on kava lactones. cis-Yangonin was also present in the herbal products.     

Visualisation of interlaboratory comparison results in PomPlots

In this work a novel graphical method is applied to the presentation of intercomparison results. This is demonstrated with the results of a recent intercomparison in measuring the ¹³⁷Cs, ⁴⁰K, and ⁹⁰Sr activity concentration in milk powder. The “PomPlot”, an intuitive graphical method, is used for producing a summary overview of the participants’ results of a common measurand. The “PomPlot” displays (relative) deviations of individual results from the reference value on the horizontal axis and (relative) uncertainties on the vertical axis.     

Complexation of gadolinium(III) ions on top of nanometre-sized magnetoliposomes

The complex of diethylenetriaminepentaacetate (DTPA) with the paramagnetic gadolinium ion [Gd(III)] is a well-known blood pool contrast agent for magnetic resonance imaging (MRI). To obtain MRI pictures from other anatomical structures, for instance from tissues containing cells with phagocytic activity, larger colloidal complexes have to be constructed. Therefore, in view of modifying the physiological behaviour, the DTPA chelate was first hydrophobized by covalently linking it to phosphatidylethanolamine (PE), and the resulting conjugate was then incorporated into nanometre-sized, sonicated phospholipid vesicles. Qualitative information on the affinity of the PE–DTPA derivative for Gd(III) ions was derived from competition experiments using the dye Arsenazo. Furthermore, it was found that only the membranotropic adducts residing in the outer shell of the vesicle bilayer are accessible to the lanthanide ion. The vesicular particulate was also used as a vehicle to transport PE–DTPA into the coating of so-called magnetoliposomes which consist of nanometre-sized iron oxide cores onto which a phospholipid bilayer is strongly chemisorbed. After loading the resulting structures with Gd(III), this new type of magnetoliposome may offer unique potentialities as a novel bi-label MRI contrast medium.     

Anion recognition by alpha-arylazo-N-confused calix[4]pyrroles

The first example of substitution reaction in the free alpha-position of N-confused calix[4]pyrroles is reported: azo-coupling with various arenediazonium salts. The obtained azocompounds were used for studies of their anion-binding properties by UV-Vis spectroscopy.     

An Interference Approach to Perturbed Angular Correlation Spectroscopy

This paper recalls the formalism of H. J. Leisi, which shows an alternative way to understand Perturbed Angular Correlation Spectroscopy: as a quantum interference effect. This revised version was published online in July 2006 with corrections to the Cover Date.     

Classification of partial difference sets in Abelian groups of order $$4p^2$$

In this article we provide a complete classification of regular partial difference sets in Abelian groups of order \(4p^2\), p an odd prime. It turns out that the known examples are the only examples. These are, up to complements, the trivial examples, the PCP examples, and a sporadic example in \(\mathbb {Z}_2^2\times \mathbb {Z}_3^2\).     

Stimuli-responsive electrospun fibers and their applications

Stimuli-responsive electrospun nanofibers are gaining considerable attention as highly versatile tools which offer great potential in the biomedical field. In this critical review, an overview is given on recent advances made in the development and application of stimuli-responsive fibers. The specific features of these electrospun fibers are highlighted and discussed in view of the properties required for the diverse applications. Furthermore, several novel biomedical applications are discussed and the respective advantages and shortcomings inherent to stimuli-responsive electrospun fibers are addressed (136 references).     

The Forgotten Pyrazines: Exploring the Dakin–West Reaction

Pyrazines are an underreported class of N-heterocycles available from nitrogen-rich biomass presenting an interesting functional alternative for current aromatics. In this work, access to pyrazines obtained from amino acids by using the 90 year old Dakin–West reaction was explored. After a qualitative screening several functional proteinogenic amino acids proved good substrates for this reaction, which were successfully scaled to multigram scale synthesis of the corresponding intermediate α-acetamido ketones. Subsequently, the conditions towards pyrazine formation using δ-amino-levulinic acid were optimized, and these were employed to synthesize a relevant set of five functional dimethylpyrazines in high purity. These pyrazines can be considered a versatile toolbox of aromatic building blocks for a wide range of applications, such as in the synthesis of polymers or metal–organic frameworks.